Microstructure Evolution of sol-gel to SnO2 Thin Film

二氧化錫薄膜由溶膠－凝膠至薄膜之微結構演變

陳溪山(C. S. Chen) ； 黃炳淮(B. H. Hwang) ； 許子建(T. C. Hsu) ； 盧宏陽(H. Y. Lu)

《材料科學與工程》 34卷1期 (2002/03) Pp. 49-54

https://doi.org/10.6409/JMSE.200203.0049

摘要

本文以X光繞射、掃描式電子顯微鏡、穿透式電子顯微鏡、熱重分析儀及熱差分析儀研究由四氯化錫懸浮溶液至二氧化錫粉末及薄膜之微結構演變，樣品包含不同階段之產物如溶液、懸浮粒析出物、凝膠、乾膠、粉末及薄膜等。熱差分析結果顯示，當溶液之酸鹼值下降時，懸浮粒子更容易聚集，造成電子顯微鏡分析顯示，二氧化錫之結晶在懸浮粒析出物中已發生，遠比X光繞射所顯示者為早。X光繞射結果顯示凝膠中之高氯離子含量有促進二氧化錫結晶及NH4Cl•NH2OH結晶之效果。由於旋鍍之分散作用，使薄膜態之二氧化錫比對應之粉末態更不易結晶。

關鍵字

溶膠－凝膠 ； 薄膜 ； 粉末 ； 二氧化錫 ； 微結構

並列摘要

Microstructure evolution from colloidal solution of SnCl4•5H2O to SnO2 powder and thin film was examined using x-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscope (TEM) in addition to thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). Samples of different stages including sol, colloidal precipitates, (wet) gel, xerogel, powder and thin films were studied. The DSC results indicate that the colloidal precipitates agglomerate more readily as the pH value of the solution decreases. SnO2 crystallization in the precipitates is observed by TEM, which indicates a much earlier commencement of crystallization than that seen in the XRD patterns. XRD results also indicate an enhancement of crystallization of SnO2 and formation of NH4Cl•NH2OH crystalline phase in the gel by a high concentration of Cl(superscript -) ions. SnO2 crystallization in the coated films does not take place as readily as that in the dry powder due to the suppression of clustering by the spinning action.

並列關鍵字

Sal-gel ； Thin film ； Powder ； SnO2 ； Microstructure